CN108329472A - A kind of synthetic method of polysulfones series plastics - Google Patents
A kind of synthetic method of polysulfones series plastics Download PDFInfo
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- CN108329472A CN108329472A CN201810073323.1A CN201810073323A CN108329472A CN 108329472 A CN108329472 A CN 108329472A CN 201810073323 A CN201810073323 A CN 201810073323A CN 108329472 A CN108329472 A CN 108329472A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/20—Polysulfones
- C08G75/23—Polyethersulfones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/20—Polysulfones
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- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
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Abstract
The present invention relates to a kind of synthetic methods of polysulfones series plastics, belong to technical field of polymer materials.The synthetic method of polysulfones series plastics of the present invention, includes the following steps：Bisphenols monomer is that reaction monomers are reacted using caustic alkali or alkalescent salt as acid binding agent using low boiling-point and polarity organic matter as solvent with dihalo benzene compound；Under nitrogen protection, constant temperature polymerize 28 hours, reacts and terminates when viscosity reaches target viscosities in kettle；Then, material is pressed into coarse filter, then is pressed into accurate filter；Filtered polymer fluid is injected in the polymer fluid receiving tank of spraying device, and at 100~150 DEG C, the tiny drop that sprayer continuously sprays is fallen into freely falling body in the precipitation solvent slot with stirring, forms uniformly tiny disk for nitrogen protection, heat preservation；Filtering, dry, packaging.Technical solution of the present invention effectively reduces the content of ashes in product.
Description
Technical field
The present invention relates to a kind of synthetic method of polysulfones series plastics, be specifically related to polysulfones (PSU), polyether sulfone (PES),
The synthetic method of polyphenylsulfone (PPSU) high molecular material, belongs to technical field of polymer materials.
Background technology
Polysulfones is high molecular polymer, is a kind of amorphous, thermoplastic resin.Its characteristic is：Excellent in mechanical performance, Gao Gang
Property, wear-resisting, acid and alkali-resistance, solvent resistant and excellent electric property etc., due to its good characteristic, polysulfones has been widely used
In the high-end zone material such as medical instrument, space flight and aviation, electronics.
Chinese patent 201310018193.9 discloses a kind of high pressure synthesis method of aromatic series polysulfone resin, polymerization pressure
Power is in 2.0~3.0MPa ranges；Constant temperature stops reaction in 6 hours.Polymerization reaction system is molecule chain growth with strand chain rupture simultaneously
The system deposited.In its polymerization reaction system, since reaction pressure is larger, strand chain rupture speed is caused to be more than molecule chain growth
Speed causes molecular weight distribution wide, is unfavorable for application of the polymer in terms of film.
Chinese patent 201510105190.8 discloses a kind of industrialized preparing process of polysulfones, its main feature is that：Polymerization knot
Solution in solvent kettle is quantified after beam, is continuously squeezed into thin film evaporation unit, thin film evaporation unit stomach wall shape of the solution in heating
Solvent is sent out at film and rapid steaming.The condensed device of solvent of evaporation enters in solvent recovery unit, and recovered solvent can be direct
In polymerisation for next time, without processing.It evaporates the polymer after solvent and forms solid in thin film evaporation unit stomach wall, Gu
Body forms powder under the stirring action for scraping wall form.It closes object powder and enters comminutor through thin film evaporation unit bottom pipeline.Though
It so solves the problems, such as massive laundering, but still needs to be granulated, the reduction of product quality can be still caused in granulation process.
Chinese patent 201710116974.X discloses a kind of sulfone Type of Collective object industrialization blowing dispersing technology, feature
It is：Sulfone Type of Collective object after reaction, identical with polymerization solvent polymerization solvent is added, it is warm to reduce reaction
Degree terminates polymerisation, reduces reaction fluid viscosity；Always it is filled with inert gas in kettle and carries out protection against oxidation；By sulfone Type of Collective
Object is slowly discharged in dispersion sieve plate, and the polymer after sieve forms drops in freely falling body and falls into equipped with dispersant band
In the dispersion slot of blender, polymer solvent is dissolved in deionized water dispersant, after blowing disperses, passes through dispersion slot bottom
The sieve discharge deionized water dispersant and polymerization solvent mixed solution in portion；Washing.The method has the following problems：When
Sulfone Type of Collective object is slowly discharged in dispersion sieve plate, this speed is not suitable for industrialized production and application, and is stopped in sieve plate
Process time is long, cannot get the protection of inert gas, and material color is deteriorated；Second is that polymer forms water in freely falling body
Drop-wise is simultaneously fallen into the dispersion slot equipped with dispersant belt stirrer, this process time is long, and polymer fluid temperature is unable to control, and is made
Increase at solution viscosity, cause the drop of freely falling body excessive or form strip, is easy the inorganic salt particle of package and mechanical admixture,
And it can not remove.
To sum up, the postprocessing working procedures of existing polysulfones preparation method need to remove inorganic salts and reaction dissolvent with a large amount of washing, and
The inorganic salts being wrapped in polysulfones particle are difficult removal, cause finished product content of ashes 0.2% or more, cause product purity not
Height influences its application in high-precision industry.And the waste water of high COD can be also brought, wastewater treatment is costly, will also result in
The pollution of environment.
Invention content
The present invention is exactly in order to which the product purity for solving existing method production is not high and wastewater treatment is costly, can cause
The technical issues of pollution of environment, provide it is a kind of can effectively remove impurity, reduce reaction product content of ashes, solve product matter
Measure the synthetic method of low polysulfones series plastics.
Polysulfones series of the present invention, including：Polysulfones (PSU), polyether sulfone (PES) and polyphenylsulfone (PPSU).
For this purpose, the present invention provides a kind of synthetic method of polysulfones series plastics, include the following steps：The first step：Bisphenols
Monomer is that reaction monomers are with caustic alkali or alkalescent salt using low boiling-point and polarity organic matter as solvent with dihalo benzene compound
Acid binding agent, nitrogen are replaced 2-4 times, and under nitrogen protection, heating makes temperature in the kettle reach 120~140 DEG C, and uses toluene or diformazan
Benzene distills 2 hours as water entrainer；Heating so that temperature in the kettle is reached 140~300 DEG C, in kettle nitrogen pressure reach 0.01~
2.0MPa, constant temperature polymerize 2-8 hours, react and terminate when viscosity reaches target viscosities in kettle.Second step：After reaction, right
Polymer fluid carries out thermal air pressure filtration, and material is first pressed into (aperture in coarse filter：0.1~2mm), then it is pressed into accurate filter (hole
Diameter：3~5 μm).Third walks：In filtered polymer fluid injection polymer fluid receiving tank, polymer fluid receiving tank need nitrogen protection,
100~150 DEG C are maintained at, polymer fluid receiving tank is equipped with sprayer, and the tiny drop that sprayer continuously sprays is in freely falling body
It falls into the precipitation solvent slot with stirring, forms uniformly tiny disk.4th step：Filtering, alcohols solvent or water washing 1~
It is 2 times, dry, packaging.
Preferably, described in the first step nitrogen replace, first extraction gas reactor to vacuum degree reach -0.08MPa with
Under, being passed through nitrogen makes pressure in kettle rise to 0.0MPa or more, and such nitrogen is replaced 2~4 times.
Preferably, caustic alkali described in the first step is selected from sodium hydroxide, potassium hydroxide, mole dosage and bisphenols monomer
Molar ratio is at (2.2-2.85):1 range.
Preferably, alkalescent salt described in the first step is selected from sodium carbonate, potassium carbonate, and mole dosage is rubbed with bisphenols monomer
That ratio is at (1.2-1.55):1 range.
Preferably, bisphenols monomer described in the first step is selected from bisphenol-A, bisphenol S, hydroquinone, '-biphenyl diphenol.
Preferably, phenyl-dihalide described in the first step is selected from 4,4-dichlorodiphenyl sulfone, 4,4- difluorodiphenyl sulfones.
Preferably, the molar ratio of bisphenols monomer and phenyl-dihalide described in the first step is (0.95-1):1.
Preferably, the dosage of first step solvent is：The dosage (volume rises) and the molar ratio of bisphenols monomer of solvent exist
(1.6-2.3)：1 range, preferably (1.8-2.3)：1.
Preferably, first step low boiling-point and polarity organic matter is that solvent is selected from dimethyl sulfoxide (DMSO), n,N-Dimethylformamide, N,
N- dimethylacetylamides, N-Methyl pyrrolidone.
Preparation method of the present invention, the product obtained are a kind of uniform tiny, thin disks, wash and are easy removing nothing
Machine salt particle.It solves traditional preparation methods to need to crush, and gained grain size thickness is uneven, fine powder when easily causing filtering
It is lost in, the blocking of strainer；And inorganic salt particle the problem of being difficult to remove wrapped up in polymer.Technical solution of the present invention is effective
The content of ashes in product is reduced, product quality is improved.There is purity using polysulfones high molecular material produced by the invention
High, the advantages that performance is stable, at low cost, pollution-free, it can be applied to the high-end zone material such as medical instrument, space flight and aviation, electronics.
Specific implementation mode
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without this hair described in claims should will not be limited
It is bright.
Embodiment 1
210 kilograms of 4,4- dichloro diphenyl sulfones, 183 kilograms of bisphenol S, potassium hydroxide 90 are added in 2500L polymerization reaction kettles
Kilogram, solvent n,N-dimethylacetamide 1500L, dimethylbenzene 100L.Be evacuated in kettle≤- 0.08MPa after, being passed through nitrogen makes
Pressure reaches >=0.00MPa in kettle, after nitrogen displacement three times, is warming up to 140 DEG C, uses dimethylbenzene as water entrainer distillation 2 hours,
Nitrogen is then passed to pressure 0.8MPa, is warming up to 190 DEG C, pressure keeps 0.5MPa, is kept for 6 hours.When polyether sulfone reaches ratio
When molten viscosity 0.53dl/g, reaction terminates.Bottom bottom valve is opened, hot pressing filter is carried out, temperature is kept for 100 DEG C.Material is pressed into pressure
(aperture in coarse filter：0.1-2mm), then it is pressed into accurate filter (aperture：3~5 μm).Filtered polymer fluid injection polymerization
In liquid receiving tank, polymer fluid receives pot bottom and is equipped with compression sprayer, and the tiny drop that compression sprayer sprays is in freely
Falling bodies shape is fallen into the sink with stirring, forms uniformly tiny disk.Filtering, then wash 1~2 time, filtering, dry, packaging.
Polyether sulfone (PES) product is obtained, ash content is 0.008% after testing, heat distortion temperature 203 DEG C (1.82MPa).
Embodiment 2
Dimethyl sulfoxide (DMSO) 1200L, 160 kilograms of bisphenol-A, 4,4-dichlorodiphenyl sulfone are added in 2500L polymerization reaction kettles
201 kilograms, 80 kilograms of sodium hydroxide, dimethylbenzene 100L.Be evacuated in kettle≤- 0.08MPa after, being passed through nitrogen makes pressure in kettle
Reach >=0.00MPa and be warming up to 140 DEG C after nitrogen displacement three times, uses dimethylbenzene to be distilled 2 hours as water entrainer, then pass to
Nitrogen is warming up to 180 DEG C of pressure and keeps 0.5MPa, kept for 4 hours to pressure 0.5MPa.When polysulfones reaches target than molten viscosity
When 0.63dl/g, reaction terminates.Bottom bottom valve is opened, hot pressing filter is carried out, temperature is kept for 100 DEG C.Material is pressed into pressure coarse filtration
(aperture in device：0.1-2mm), then it is pressed into accurate filter (aperture：3~5 μm).Filtered polymer fluid injection polymer fluid receives
In tank, polymer fluid receives pot bottom and is equipped with compression sprayer, and the tiny drop that compression sprayer sprays is in freely falling body shape
It falls into the methanol slot with stirring, forms uniformly tiny disk.Filtering, again with methanol are washed 1~2 time, filtering, dry, packet
Dress.Obtain polysulfones (PSU) product, ash content 0.01%, heat distortion temperature 175 DEG C (1.82MPa).
Embodiment 3
210 kilograms of 4,4- dichloro diphenyl sulfones, 183 kilograms of bisphenol S, sodium carbonate 120 are added in 2500L polymerization reaction kettles
Kilogram, solvent N-methyl pyrilidone 1200L, dimethylbenzene 100L.Be evacuated in kettle≤- 0.08MPa after, being passed through nitrogen makes kettle
Interior pressure reaches >=0.00MPa and is warming up to 140 DEG C after nitrogen displacement three times, uses dimethylbenzene as water entrainer distillation 2 hours, so
After be passed through nitrogen to pressure 0.8MPa, be warming up to 200 DEG C, pressure keeps 0.5MPa, is kept for 6 hours.When polyether sulfone reaches than molten
When viscosity 0.58dl/g, reaction terminates.Bottom bottom valve is opened, hot pressing filter is carried out, temperature is kept for 100 DEG C.It is thick that material is pressed into pressure
In filter (aperture 0.1-2mm), then it is pressed into accurate filter (aperture：3~5 μm).Filtered polymer fluid injects polymer fluid
In receiving tank, polymer fluid receives pot bottom and compression sprayer is housed, and the tiny drop that compression sprayer sprays is in freely falling body
Shape is fallen into the water with stirring, forms uniformly tiny disk.Filtering, then 95% ethyl alcohol wash 1~2 time, filtering, dry, packet
Dress.Obtain polyether sulfone (PES) product, ash content 0.012%, heat distortion temperature 203 DEG C (1.82MPa).
Embodiment 4
211 kilograms of 4,4- dichloro diphenyl sulfones, 80.9 kilograms of hydroquinone, sodium carbonate are added in 2500L polymerization reaction kettles
100 kilograms, solvent n,N-dimethylacetamide 1325L, dimethylbenzene 100L.After nitrogen displacement three times, 140 DEG C are warming up to, with two
Toluene distills 2 hours as water entrainer, then passes to nitrogen to pressure 0.8MPa, is warming up to 190 DEG C, and pressure keeps 0.5MPa,
It is kept for 6 hours.When polysulfones reaches than molten viscosity 0.50dl/g, reaction terminates.Bottom bottom valve is opened, hot pressing filter, temperature are carried out
Kept for 90 DEG C.Material is pressed into pressure coarse filter (hole 0.1-2mm), then is pressed into accurate filter (aperture：3~5 μm).Filtering
In polymer fluid injection polymer fluid receiving tank afterwards, polymer fluid receives pot bottom and compression sprayer is housed, what compression sprayer sprayed
Tiny drop is fallen into freely falling body shape in the ethyl alcohol with stirring, forms uniformly tiny disk).Filtering, then washed with ethyl alcohol
It washs 1~2 time, filtering, dry, packaging.Obtain polyphenylene oxide sulfone product, ash content 0.009%, 175 DEG C of heat distortion temperature
(1.82MPa)。
Embodiment 5
203 kilograms of 4,4- difluorodiphenyls sulfone, 149 kilograms of '-biphenyl diphenol, sodium carbonate are added in 2500L polymerization reaction kettles
103 kilograms, solvent dimethyl sulfoxide (DMSO) 850L, toluene 100L.After nitrogen displacement three times, 140 DEG C are warming up to, uses toluene as band water
Agent is distilled 2 hours, is then passed to nitrogen to pressure 0.8MPa, is warming up to 190 DEG C, pressure keeps 0.5MPa, is kept for 5 hours.It is poly-
When benzene sulfone reaches target than molten viscosity 0.43dl/g, reaction terminates.Bottom bottom valve is opened, hot pressing filter is carried out, temperature is kept for 90 DEG C.
Material is pressed into pressure coarse filter (hole 0.1-2mm), then is pressed into accurate filter (aperture：3~5 μm).Filtered polymerization
Liquid injects in polymer fluid receiving tank, and polymer fluid receives pot bottom and compression sprayer, the tiny liquid that compression sprayer sprays are housed
Drop is fallen into freely falling body shape in the ethyl alcohol with stirring, forms uniformly tiny disk).Filtering, then wash 1~2 with ethyl alcohol
It is secondary, filtering, dry, packaging.Obtain polyphenylene oxide sulfone product, ash content 0.006%.Heat distortion temperature 207 DEG C (1.82MPa).
Claims (9)
1. a kind of synthetic method of polysulfones series plastics, characterized in that include the following steps：
The first step：Bisphenols monomer is reaction monomers with dihalo benzene compound, using low boiling-point and polarity organic matter as solvent, with severe
Property alkali or alkalescent salt be acid binding agent, nitrogen replace 2~4 times after, under nitrogen protection, heating so that temperature in the kettle is reached 120~140
DEG C, and toluene or dimethylbenzene is used to be distilled 2 hours as water entrainer, then 190~300 DEG C are warming up to, nitrogen pressure reaches in kettle
0.01~2.0MPa, constant temperature polymerize 2-8 hours, react and terminate when viscosity reaches target viscosities in kettle；The low boiling-point and polarity
Organic matter is that solvent is selected from dimethyl sulfoxide (DMSO), N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone；
Second step：After reaction, thermal air pressure filtration is carried out to polymer fluid, the coarse filtration for being first 0.1-2mm by material indentation aperture
In device, then it is pressed into the accurate filter that aperture is 3~5 μm；
Third walks：In filtered polymer fluid injection polymer fluid receiving tank, nitrogen protection is maintained at 100~150 DEG C, gathers
It closes liquid receiving tank and sprayer is housed, the tiny drop that sprayer continuously sprays falls into molten with the precipitation stirred in freely falling body
In agent slot, uniformly tiny disk is formed；
4th step：Filtering, alcohols solvent or water washing 1~2 time, dry, packaging.
2. the synthetic method of polysulfones series plastics according to claim 1, it is characterised in that the nitrogen of the first step is protected
Shield, extraction gas reactor to vacuum degree reaches -0.08MPa first makes pressure in kettle rise to 0.0MPa hereinafter, being passed through nitrogen
More than, after such nitrogen is replaced 2~4 times, under nitrogen protection, heating makes temperature in the kettle reach 140 DEG C, and uses toluene or diformazan
Benzene distills 2 hours as water entrainer.
3. the synthetic method of polysulfones series plastics according to claim 1, it is characterised in that in the first step, toluene or
After dimethylbenzene band water, then being warming up to 190-300 DEG C and being passed through high pure nitrogen makes in kettle pressure reach 0.01~2.0MPa, constant temperature
Polymerization 2-8 hours is reacted when viscosity reaches target viscosities in kettle and is terminated.
4. the synthetic method of polysulfones series plastics according to claim 1, it is characterised in that in the first step, caustic alkali
Selected from sodium hydroxide, potassium hydroxide, mole dosage：The mole dosage ratio of bisphenols monomer is (2.2-2.85)：1.
5. the synthetic method of polysulfones series plastics according to claim 1, it is characterised in that in the first step, alkalescent
Salt is selected from sodium carbonate, potassium carbonate, mole dosage：The mole dosage ratio of bisphenols monomer is (1.2-1.55)：1.
6. the synthetic method of polysulfones series plastics according to claim 1, it is characterised in that in the first step, bisphenols
Monomer is selected from bisphenol-A, bisphenol S, hydroquinone, '-biphenyl diphenol；The phenyl-dihalide is selected from 4,4- dichloro diphenyl sulfones, 4,4- difluoros
Diphenyl sulphone (DPS).
7. the synthetic method of polysulfones series plastics according to claim 1, it is characterised in that in the first step, bisphenols
The molar ratio of monomer and phenyl-dihalide is (0.95-1):1.
8. the synthetic method of polysulfones series plastics according to claim 1, it is characterised in that in the first step, solvent
Dosage is：The volumetric usage of solvent is with the molar ratio of bisphenols monomer at (1.6-2.3)：1 range, the volumetric usage of the solvent
Unit is to rise.
9. the synthetic method of polysulfones series plastics according to claim 1, it is characterised in that in the first step, solvent
Dosage is：The volumetric usage of solvent is with the molar ratio of bisphenols monomer at (1.8-2.3)：1 range, the volumetric usage of the solvent
Unit is to rise.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662453A (en) * | 2020-06-30 | 2020-09-15 | 富海(东营)新材料科技有限公司 | Method for preparing polysulfone resin material by adopting cooperative dehydration process |
| CN112300392A (en) * | 2020-11-09 | 2021-02-02 | 江西金海新能源科技有限公司 | Antibacterial sulfone polymer and preparation method and application thereof |
| CN112679631A (en) * | 2020-12-22 | 2021-04-20 | 宁波南大光电材料有限公司 | Method for removing small molecular substances in synthetic resin |
| CN113637168A (en) * | 2021-09-22 | 2021-11-12 | 山东海科创新研究院有限公司 | Preparation method of sulfone polymer |
| CN113881044A (en) * | 2021-10-29 | 2022-01-04 | 杭州润森化妆品包装有限公司 | High-temperature-resistant cosmetic bottle cap and preparation method thereof |
| CN114106330A (en) * | 2021-12-31 | 2022-03-01 | 南京清研新材料研究院有限公司 | Preparation process and device of bisphenol A type polysulfone resin and modified material thereof |
| CN114656638A (en) * | 2022-03-03 | 2022-06-24 | 万华化学集团股份有限公司 | Method and device for continuously synthesizing polysulfone |
| WO2022135184A1 (en) * | 2020-12-21 | 2022-06-30 | 富海(东营)新材料科技有限公司 | Industrial purification process and device for polysulfone resin material |
| CN116478403A (en) * | 2023-04-07 | 2023-07-25 | 安徽卓润新材料科技有限公司 | Polysulfone resin production process and polysulfone resin production system |
| CN117362648A (en) * | 2023-11-15 | 2024-01-09 | 山东浩然特塑股份有限公司 | Method for preparing polysulfone resin by segmented polymerization |
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| CN111662453A (en) * | 2020-06-30 | 2020-09-15 | 富海(东营)新材料科技有限公司 | Method for preparing polysulfone resin material by adopting cooperative dehydration process |
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| CN113637168A (en) * | 2021-09-22 | 2021-11-12 | 山东海科创新研究院有限公司 | Preparation method of sulfone polymer |
| CN113881044A (en) * | 2021-10-29 | 2022-01-04 | 杭州润森化妆品包装有限公司 | High-temperature-resistant cosmetic bottle cap and preparation method thereof |
| CN114106330A (en) * | 2021-12-31 | 2022-03-01 | 南京清研新材料研究院有限公司 | Preparation process and device of bisphenol A type polysulfone resin and modified material thereof |
| CN114656638A (en) * | 2022-03-03 | 2022-06-24 | 万华化学集团股份有限公司 | Method and device for continuously synthesizing polysulfone |
| CN116478403A (en) * | 2023-04-07 | 2023-07-25 | 安徽卓润新材料科技有限公司 | Polysulfone resin production process and polysulfone resin production system |
| CN116478403B (en) * | 2023-04-07 | 2024-03-26 | 安徽卓润新材料科技有限公司 | Polysulfone resin preparation method and preparation device thereof |
| CN117362648A (en) * | 2023-11-15 | 2024-01-09 | 山东浩然特塑股份有限公司 | Method for preparing polysulfone resin by segmented polymerization |
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